Apparatus for conditioning lyophilised products

ABSTRACT

This invention relates to apparatus for conditioning a lyophilised product under atmospheric pressure in an enclosure linked to a pumping unit and lyophilisation is effected under vacuum. The enclosure is associated with means for moving a stopper adapted hermetically to block a neck on the enclosure, and this means is adapted to enable the stopper to move on both sides of the blocked position, viz: to a withdrawal position within the enclosure or to a separation position outside the enclosure in an extension of the neck. The neck includes means for attachment to various accessories in a sealed manner.

United States Patent [191 Duprai et a1.

[ 51 Feb. 5, 1974 Procedes Georges Claude, Paris, France [22] Filed: Aug. 13, 1971 [21] Appl. No: 171,682

[30] Foreign Application Priority Data Aug. 18, 1970 France 7039335 [52] US. Cl. 34/92, 34/5 [51] Int. Cl. F26b 5/06, F26b 13/30 [58] Field of Search... 34/5, 15, 92; 53/319; 141/65,

[56] References Cited UNITED STATES PATENTS 3,286,366 11/1966 Seligman ..34/92 2,198,752 4/1940 Barr 34/5 X 3,616,543 11/1971 Barclay 34/15 X 3,474,543 10/1969 Bender et a1. 34/92 X FOREIGN PATENTS OR APPLICATIONS 701,888 l/1954 Great Britain 34/5 Primary Examiner-William F. ODea Assistant ExaminerWilliam C. Anderson Attorney, Agent, or F irm- Browdy and Neimark [5 7] ABSTRACT This invention relates to apparatus for conditioning a lyophilised product under atmospheric pressure in an enclosure linked to a pumping unit and lyophilisation is effected under vacuum. The enclosure is associated with means for moving a stopper adapted hermetically to block a neck on the enclosure, and this means is adapted to enable the stopper to move on both sides of the blocked position, viz: to a withdrawal position within the enclosure or to a separation position outside the enclosure in an extension of the neck. The neck includes means for attachment to various accessories in a sealed manner.

5 Claims, 6 Drawing Figures Patented Feb. 5, 1974 2 Sheets-Sheet. 1

M, W ja W Patented Feb. 5, 1974 3,789,515

2 Sheets-Sheet 2 APPARATUS FOR CONDHTHONING LYOPHILISED PRODUCTS The present invention relates to apparatus for conditioning lyophilised products under atmospheric pressure, and is more particularly applicable to a rotary lyophilisation machine.

It is now known to effect in succession congealing and lyophilisation of products to be dried in a common rotary enclosure.

It is often necessary for the products to be treated and conditioned under an aseptically inert atmosphere and without contact with the air.

The invention has for an object the provision of means for carrying out a method of conditioning a lyophilised product under atmospheric pressure, applicable more particularly to the use of a rotary lyophilisation machine of the kind comprising a lyophilisation enclosure containing the treated product, and linked to a pumping unit, wherein, after achieving lyophilisation under vacuum and breaking of the vacuum by introducing an inert gas into the enclosure, in a blocking phase, the enclosure is hermetically sealed, a storage receptacle also filled with an inert gas is attached thereto in sealed manner, the link is established between the receptacle and the enclosure, the lyophilised product is transferred by gravity from the enclosure to the receptacle, then in a separation phase the said receptacle is hermetically closed and is then separated from the enclosure.

It is thus possible to condition lyophilised products under an inert atmosphere in a substantially sterile manner.

The invention consists in a lyophilisation apparatus of the type comprising a lyophilisation enclosure, more particularly one that rotates about an axis, and removably connectible to a pumping unit by a neck centred on the said axis, wherein said enclosure is associated with means for moving a stopper adapted hermetically to block said neck, said means being adapted to enable said stopper to move on both sides of said blocking position, alternatively to a position of withdrawal within the enclosure or to a separation position, outside said enclosure, in the extension of the neck, and wherein said neck comprises means for attachment to detachable accessories in a sealed manner, more particularly to a storage receptacle which, in its position attached to the enclosure, is arranged so that said stopper in its separation position hermetically blocks the orifice of said receptacle.

In use of the apparatus, after lyophilisation has been carried out, the enclosure is closed by the stopper placed in the blocking position; it is separated from the pumping unit and a storage receptacle or a conditioner can be attached thereto. After filling the receptacle with an inert gas, the stopper is placed in the withdrawal position which enables the product in the storage receptacle to be transferred by simple gravity. The stopper is thus placed in the separation position in which it blocks the receptacle. The latter may then be separated from the enclosure.

The product has thus been conditioned without any contact with the outside air.

In order that the invention may be more clearly understood, reference will now be made to the accompanying drawings, which show one embodiment thereof by way of example only, and in which:

FIG. 1 shows a diagrammatic view of this embodiment, comprising a rotary lyophilisation enclosure, joined to a pumping unit,

FIG. 2 shows a part view of this apparatus, illustrating the blocking stage of the enclosure, lyophilisation having being assumed to be already carried out,

FIG. 3 shows how the enclosure is connected to a storage receptacle,

F IG. 4 shows the transfer of the lyophilised product to the storage receptacle, the stopper being in the withdrawal position, and

FIGS. 5 and 6 show the final stages of the process, the receptacle firstly being hermetically sealed, then closed by the stopper in the separation position and then separated from the lyophilisation enclosure.

Referring now to the drawings, in FIG. 1, the lyophilisation apparatus according to the invention primarily incorporates a rotary lyophilisation enclosure 1, containing the product to be treated, associated with rotation means (not shown) with a refrigerating or heating tank 2 in which the said enclosure is partially immersed; if desired, other heating means as schematically shown at 3, may also be provided.

The enclosure 1 comprises at one end and on the en closure axis, a neck 5 joined to one of the ends 7 of a rotary joint 8, the other end 9 of this joint being attached to a vertical cylinder 10, to which a pumping unit (not shown) is fitted at 11, condensing the water vapour resulting from subliming the treated product, in a conventional manner.

The cylinder 10 has a female flange 12, centred on the axis of rotation of the enclosure 1; various accessories can be fitted to this flange: for example, a ramp (not shown) for injecting liquid to be congealed passing through the joint 8 and into the interior of the enclosure 1; a cylinder containing a movable filter 16 which can be moved up to the enclosure 1; and a hollow rod 17 serving to position the filter 16 may also serve as a pressure collector in the enclosure 1 and is joined to a vacuum gauge head 19.

According to an essential arrangement of the invention, the end of the enclosures 1 opposite the neck 5, has an axial extension 20, providing internally a cylindrical conduit 22, centred on the axis of rotation of the enclosure, and having the same diameter as that of the internal passage 30 of the neck 5. This conduit 22 is adapted to receive a stopper 24 provided with suitable sealing joints and mounted at the end of a rod 25 which passes through a sliding joint 27 in sealed manner, positioned in a restricted end 28 of the extension 20.

When lyophilisation has been carried out and the vacuum of the enclosure has been replaced by an inert gas, the filter 16, if desired, having been replaced in the cylinder 15, the stopper 24 is moved from the conduit 22 into the passage 30 of the neck 5, which it hermetically blocks (FIG. 2). This operation is effected extremely simply by sliding the rod 25 through the joint 27.

The enclosure 1 can, therefore, be isolated from the rest of the apparatus by separating it from the rotary joint 8.

In place of the end 7 of this joint, the neck 32 of a storage receptacle 33 provided with two nozzles 36 and 37 having valves 34 and 35 respectively is fastened to the neck 5. The necks 5 of the enclosure 1 and 32 of the receptacle 33 are arranged in a manner to fit hermetically each to the other and to arrange between enclosure and receptacle an internal communication passage of the diameter of the passage 30, thus adapted to receive the stopper 24.

The receptacle 33 thus mounted, vacuum is created therein, then it is filled with the same inert gas as the enclosure 1 by operating the valves 34 and 35 (FIG. 3).

The stopper 24 is moved rearwardly into the extension 20, in the withdrawal position, which establishes the link between the enclosure 1 and the receptacle 33. By gravity, it is possible to transfer the treated product 40 to the receptacle 33 (FIG. 4).

The stopper 24 is thus pushed back into the neck 5 and moved so as to block the neck 32 of the receptacle 33, in the position of separation (FIG. 5).

Receptacle and enclosure are thus separated from each other. The rod 25 is then separated from the stopper 24. To this end, advantageously it may have a threaded end 41 engaging a threaded bore 42 of the stopper 24 (FIG. 6).

The apparatus according to the invention can be applied to lyophilisation of all products which have to be treated aseptically and out of contact with air.

We claim:

1. Apparatus for lyophilisation comprising:

a. a vessel defining a lyophilisation enclosure and rotatable about an axis of rotation passing through the center of said vessel and adapted to contain a product being treated;

b. means for rotating said vessel;

c. means for supplying heat or refrigeration to said vessel;

!. means detachably connected to said vessel for evacuating said vessel or for introducing an inert gas thereinto;

e. a first tubular neck at one end of said vessel positioned in alignment with said axis and defining a recess for storing a movable stopper member;

f. a second tubular neck at the opposite end of said vessel in alignment with said axis and with the first tubular neck providing inlet and discharge means for said vessel, and adapted to receive said stopper member with a close fit;

g. a stopper member mounted at one end of means slidably movable between said tubular necks and coaxial with said vessel axis from a storage position in the first neck to a closure position in the second neck;

h. said rod being adapted to be withdrawn through a seal at the outer end of said first neck.

2. The apparatus of claim 1 which further includes a storage receptacle detachably connected to said second neck and having an opening adapted to receive said stopper member as a closure.

3. The apparatus of claim 2 in which said stopper is detachably mounted at the end of said rod.

4. The apparatus of claim 1 in which said means for moving said stopper member consists of a rod centered along the axis of said enclosure and passing through the wall of said enclosure through said first neck through a sliding sealing joint positioned at the outer end of said neck, said stopper member being mounted at the end of the rod which extends toward the interior of said enclosure.

5. The apparatus of claim 4 in which said sliding sealing joint is mounted in said enclosure coaxially with the axis of the enclosure and is adapted to accomodate said stopper member in its storing position.

* II =l= 

1. Apparatus for lyophilisation comprising: a. a vessel defining a lyophilisation enclosure and rotatable about an axis of rotation passing through the center of said vessel and adapted to contain a product being treated; b. means for rotating said vessel; c. means for supplying heat or refrigeration to said vessel; d. means detachably connected to said vessel for evacuating said vessel or for introducing an inert gas thereinto; e. a first tubular neck at one end of said vessel positioned in alignment with said axis and defining a recess for storing a movable stopper member; f. a second tubular neck at the opposite end of said vessel in alignment with said axis and with the first tubular neck providing inlet and discharge means for said vessel, and adapted to receive said stopper member with a close fit; g. a stopper member mounted at one end of means slidably movable between said tubular necks and coaxial with said vessel axis from a storage position in the first neck to a closure position in the second neck; h. said rod being adapted to be withdrawn through a seal at the outer end of said first neck.
 2. The apparatus of claim 1 which further includes a storage receptacle detachably connected to said second neck and having an opening adapted to receive said stopper member as a closure.
 3. The apparatus of claim 2 in which said stopper is detachably mounted at the end of said rod.
 4. The apparatus of claim 1 in which said means for moving said stopper member consists of a rod centered along the axis of said enclosure and passing through the wall of said enclosure through said first neck through a sliding sealing joint positioned at the outer end of said neck, said stopper member being mounted at the end of the rod which extends toward the interior of said enclosure.
 5. The apparatus of claim 4 in which said sliding sealing joint is mounted in said enclosure coaxially with the axis of the enclosure and is adapted to accomodate said stopper member in its storing position. 